{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,4,29]],"date-time":"2026-04-29T04:43:20Z","timestamp":1777437800319,"version":"3.51.4"},"reference-count":25,"publisher":"Wiley","issue":"5","license":[{"start":{"date-parts":[[2024,3,11]],"date-time":"2024-03-11T00:00:00Z","timestamp":1710115200000},"content-version":"vor","delay-in-days":10,"URL":"http:\/\/onlinelibrary.wiley.com\/termsAndConditions#vor"}],"content-domain":{"domain":["analyticalsciencejournals.onlinelibrary.wiley.com"],"crossmark-restriction":true},"short-container-title":["J of Separation Science"],"published-print":{"date-parts":[[2024,3]]},"abstract":"<jats:p>An analytical quality by design\u2010based high\u2010performance liquid chromatography method for determining metformin (MET) and sitagliptin (SIT) in stress\u2010degraded samples was developed and validated. The analytical target profile and risk assessment\u2010driven critical method variables, for example, pH, % aqueous, and buffer concentration, were studied for their effect on method responses of retention time and resolution using a central composite design. The correlation regression coefficient was more than 0.8, and variables interaction was significant on method responses with curvature effect. The method operable design region afforded an aqueous range of 55%\u201370% and an <jats:italic>ortho<\/jats:italic>\u2010phosphoric acid buffer of 0.1% with a pH of 3.0\u20134.0 as a robust region for the suitable method performance characteristics. The separation of MET and SIT from their degradants (<jats:italic>m\/z<\/jats:italic> 85.0509; <jats:italic>m\/z<\/jats:italic> 193.0694) on the C<jats:sub>8<\/jats:sub> column was achieved using a mobile phase consisting of 0.1% <jats:italic>ortho<\/jats:italic>\u2010phosphoric acid and methanol (60:40% v\/v; pH 3.0). The optimized method eluted MET and SIT at 4.3\u00a0\u00b1\u00a00.2 and 7.1\u00a0\u00b1\u00a00.2\u00a0min, respectively, with acceptable specificity and resolution. The linearity ranges of 25\u2013250\u00a0\u03bcg\/mL (r<jats:sup>2<\/jats:sup>: 0.9982) and 5\u201350\u00a0\u03bcg\/mL (r<jats:sup>2<\/jats:sup>: 0.9989) was established for MET and SIT, respectively. The % recovery (98.81%\u2013102.17%), precision (0.55%\u20131.65%), and robustness study for method variables were acceptable.<\/jats:p>","DOI":"10.1002\/jssc.202300605","type":"journal-article","created":{"date-parts":[[2024,3,11]],"date-time":"2024-03-11T10:20:26Z","timestamp":1710152426000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":20,"title":["Analytical quality by design approach for the development of high\u2010performance liquid chromatography method for simultaneous analysis of metformin and sitagliptin in the presence of major degradation products"],"prefix":"10.1002","volume":"47","author":[{"given":"Rajesh","family":"Pawar","sequence":"first","affiliation":[{"name":"Department of Pharmaceutical Analysis National Institute of Pharmaceutical Education and Research (NIPER) Hajipur  Bihar India"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-7956-3276","authenticated-orcid":false,"given":"Pothuraju","family":"Naresh","sequence":"additional","affiliation":[{"name":"Department of Pharmaceutical Analysis National Institute of Pharmaceutical Education and Research (NIPER) Hajipur  Bihar India"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Bhadrayya","family":"Kalva","sequence":"additional","affiliation":[{"name":"Swaroop Tech Services Private Ltd  Hyderabad India"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"M. 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